Acetic Acid → HCID 178481542、化合物

HRID 2258473ノート

反応式

HRID 2258473 の反応式
N[C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1.Cl.C(O)(=[O:20])C>>[OH:20][C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1

参加物

4

反応物 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 16492566-Amino-3-methyl-1-phenylpyrimidine-2,4(1H,3H)-dione

生成物 1

HCID 178481542HCID 178481542、化合物収率 68%

反応条件

温度
100 °C

実験手順

6-Amino-3-methyl-1-phenyluracil as obtained in Reference Example 1 (8.7 g, 40 mM) was dissolved in 80 ml of acetic acid and hydrochloric acid (16 ml) was added, followed by heating at 100° C. for 1 hour. The solvent acetic acid was then distilled off under reduced pressure and water war added to the residue. The pH of the resulting solution was adjusted to 1 by adding hydrochloric acid and a product was extracted with dichloromethane. After the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol was performed to give 6-hydroxy-3-methyl-1-phenyluracil (yield: 5.9 g, or 68% based on 6-amino-3-methyl-1-phenyluracil).

後処理

  1. distillationThe solvent acetic acid was then distilled off under reduced pressure and water war
  2. additionadded to the residue
  3. additionby adding hydrochloric acid
  4. extractiona product was extracted with dichloromethane
  5. distillationAfter the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol

出典と根拠

ORDレコード
ord-05a1dbe9acbc41669f9f1ebfef38eac1
出典データセット
uspto-grants-1997_08
特許番号
US05661153

反応ノート

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